WO2023077790A1 - Outil et procédé pour l'incorporation interne et externe de poudre et l'infiltration de silicium fondu d'un composant composite 2d, 3dn à matrice céramique - Google Patents

Outil et procédé pour l'incorporation interne et externe de poudre et l'infiltration de silicium fondu d'un composant composite 2d, 3dn à matrice céramique Download PDF

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WO2023077790A1
WO2023077790A1 PCT/CN2022/096447 CN2022096447W WO2023077790A1 WO 2023077790 A1 WO2023077790 A1 WO 2023077790A1 CN 2022096447 W CN2022096447 W CN 2022096447W WO 2023077790 A1 WO2023077790 A1 WO 2023077790A1
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graphite
crucible
ceramic matrix
matrix composite
nozzle
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PCT/CN2022/096447
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Chinese (zh)
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史思涛
苏海龙
王鹏
张少博
张倩
康志杰
李仁意
宋海龙
马文科
杨攀
赵盟辉
赵兵兵
何江怡
付志强
李丹
刘澍雨
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西安鑫垚陶瓷复合材料有限公司
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details specially adapted for crucible or pot furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details specially adapted for crucible or pot furnaces
    • F27B14/0806—Charging or discharging devices
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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    • C04B2235/428—Silicon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
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    • F27B14/00—Crucible or pot furnaces
    • F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
    • F27B2014/045—Vacuum

Definitions

  • the invention relates to continuous fiber-reinforced silicon carbide ceramic matrix composite material fusion siliconization modification, in particular to an inner/outer embedded powder fusion siliconization tooling and method suitable for 2D and 3DN ceramic matrix composite composite components.
  • Continuous carbon fiber reinforced ceramic matrix composites (Continuous Fiber Reinforced Ceramic Matrix Composites, CFCC) inherits the excellent characteristics of ceramics such as low density, high strength and oxidation resistance, and overcomes the weaknesses of ceramic brittleness and poor reliability.
  • the fracture behavior of metals which is insensitive to cracks and not prone to catastrophic fractures, has great application potential in the aerospace field.
  • carbon fiber toughened silicon carbide ceramic matrix composites which combine the advantages of C/C composites and SiC ceramics, can meet the long-term use in an aerobic environment below 1650°C, the limited life below 2000°C and the instantaneous life below 2800°C usage requirements.
  • C/SiC composite materials have a series of excellent properties such as high specific strength, high specific modulus, ablation resistance, high temperature resistance and low density, and are currently one of the most potential thermal protection system materials.
  • the preparation process of thermal structural composites can be divided into: gas phase route, also known as chemical vapor infiltration (CVI); liquid phase route, including polymer impregnation pyrolysis (PIP) and liquid silicon infiltration (LSI) or reactive melt infiltration process (RMI).
  • the different components of the composite material that is, the interface phase, the matrix and the outer coating, can be continuously deposited from the gaseous precursor under the condition of medium temperature, low pressure or normal pressure of 900-1000 ° C by using the gas phase route.
  • preform densification (CVI) the interfacial phase and SiC matrix are deposited onto the fiber surfaces inside the pores of the preform.
  • the CVI process has the following outstanding advantages: strong practicability, low preparation temperature, effective realization of composition design of composite materials on the microscopic scale, suitable for the preparation of high fiber volume fraction, For products with complex shape, net size and wide range of sizes, the preparation process has little damage to the fiber.
  • the RMI process is a densification process that generates a matrix in situ through a chemical reaction, and the reaction products are usually carbides and borides. Its principle is to realize the introduction of carbides and borides through the reaction of high-temperature molten metal elements or alloy mixtures with porous materials containing carbon or boron. There is no need to apply additional mechanical pressure during the RMI process, and the molten metal or alloy spontaneously infiltrates into the interior of the preform under the action of capillary force, and reacts with carbon or the introduced precursor to form a ceramic matrix.
  • the carbon or precursor in the porous material can be derived from the prefabricated body matrix itself (such as C/C composite material), or the carbon phase can be introduced into the porous prefabricated body by slurry infiltration method or PIP method.
  • the RMI process has low preparation cost and short production cycle, and can realize the preparation of components with complex shapes.
  • the prepared material has low residual porosity, good compactness and excellent thermal conductivity.
  • the RMI process also has some disadvantages: during the impregnation reaction, if it is not protected, the carbon fiber will react with the impregnated metal phase, corrode and damage the fiber, and affect the mechanical properties of the material.
  • CVI process can be used to first prepare C/C preform with a certain density, and then react with molten Si at high temperature.
  • the CVI method can also be used to prepare porous C/SiC composites with a certain density, and then the resin is introduced into the porous C/SiC by the slurry infiltration method to crack and generate excess carbon, and then the RMI reaction is carried out to introduce molten Si into the composite material to obtain C/SiC composite material with high density.
  • the pre-deposited SiC matrix can effectively protect the carbon fiber by SiC.
  • the carbon fiber will not be corroded by the Si melt, and the load-carrying capacity of the carbon fiber can be better exerted. Therefore, the RMI method is often used to prepare components such as aircraft engine tail nozzle walls. .
  • a single large-size circular cross-section three-dimensional needle-punched nozzle prefabricated body (referred to as 3DN nozzle prefabricated body) has a mature process for RMI modification of ceramic matrix composite components.
  • the process route is briefly described as follows:
  • Embed modified powder on the outside of the 3DN nozzle prefabrication body with a certain density and porosity and complete the RMI process of the three-dimensional acupuncture nozzle prefabrication body through a certain temperature system, and complete the high-temperature modified 3DN nozzle prefabrication body Assembly with two-dimensional laminated parts (2D parts) (such as end flanges, corner boxes, etc.) followed by finishing and other subsequent processes.
  • 2D parts two-dimensional laminated parts
  • the three-dimensional acupuncture preform needs to reserve processing capacity before RMI, and the preform hardness after RMI siliconizing is extremely high (the modified product is mainly silicon carbide, with a Mohs hardness of 9.5), mechanical processing The performance is very poor, which will bring great difficulties to the subsequent processing and assembly process.
  • the two-dimensional laminated reinforcement member is eroded by molten silicon liquid, the interlayer bonding force is greatly reduced, and the mechanical properties are deteriorated;
  • the purpose of the present invention is to solve the problem of 2D parts being easily eroded by silicon melt and causing performance degradation in the RMI process of large-size circular cross-section 3DN nozzle prefabrication in 2D and 3DN ceramic matrix composite components, and the prefabrication of 2D parts and 3DN nozzles.
  • the high-temperature modification of the 3DN nozzle prefabricated body at the body contact surface, the process difficulty of overall densification of the components, and the technical problem that the 3DN nozzle prefabricated body is easily deformed during the modification process the present invention provides a 2D, 3DN ceramic matrix composite material Fused silicon infiltration tooling and method for embedded powder inside and outside components.
  • a 2D, 3DN ceramic matrix composite component internal and external powder-embedded fused siliconization tooling which is special in that it includes a crucible, 2D parts graphite protection tooling, graphite column, graphite support sheet, graphite inner support and composite material deformation control tooling, And the second annular graphite paper stack, the third annular graphite paper stack and (N-1) first annular graphite paper stacks; said N ⁇ 3;
  • the crucible adopts a combined graphite crucible, which is composed of N graphite crucible layers.
  • Each graphite crucible layer is stacked coaxially from bottom to top, and is defined as the 1st, 2nd, ..., N crucible layers from the bottom to the top.
  • the shape of the crucible cavity matches the shape of the 2D and 3DN ceramic matrix composite components, and the inner diameter of the crucible cavity at each height is greater than the outer diameter of the corresponding height of the 2D and 3DN ceramic matrix composite components;
  • the graphite protective tooling of the 2D parts is arranged at the bottom of the crucible cavity, including the graphite ring wall, the graphite ring plate arranged at the inner bottom of the graphite ring wall, and the graphite ring wall and the bottom of the graphite ring plate are correspondingly arranged and evenly distributed along the circumference.
  • the inner diameter of the graphite ring plate is greater than the outer diameter of the graphite column and less than the outer diameter of the 2D part b in the 2D and 3DN ceramic matrix composite assembly; the height of the graphite ring wall is higher than the height of the 2D part b;
  • the area between adjacent leg groups is used as a slurry via hole;
  • the graphite column is coaxially arranged in the crucible cavity, and its bottom end is in contact with the inner bottom surface of the crucible through the graphite ring plate, and its diameter is smaller than that of 2D and 3DN ceramic substrates.
  • the inner diameter of the small end of the 3DN nozzle prefabricated body a in the composite material component, and the top is provided with a cross groove;
  • the graphite holder is arranged on the lower side of the graphite column;
  • the graphite inner holder is a variable-diameter ring with a bottom hole, and its outer diameter is smaller than the inner diameter of the 3DN nozzle prefabricated body a, and the graphite inner holder passes through the bottom circle
  • the hole is set on the graphite column, the diameter of the bottom hole is equal to the outer diameter of the graphite column, and the bottom of the graphite inner support is supported by the graphite support;
  • the composite material deformation control tool is a cross plate, the material of which is the same as that of the 2D and 3DN ceramic matrix composite components, and its density is greater than that of the 2D and 3DN ceramic matrix composite components, and the middle part of the cross plate is embedded in the In the cross groove, a flat groove is provided on the lower surface of each end;
  • the first annular graphite paper laminate is an annular graphite paper laminate in which multiple layers of graphite paper are stacked and bonded together; (N-1) first annular graphite paper laminates are respectively laid on the inner cavity of the crucible and the 3DN nozzle Between the outer walls of the prefabricated body a, it is used as a layered baffle for the filler; the outer diameter of each first annular graphite paper laminate is equal to the corresponding height of the crucible cavity and the inner diameter of the truncated circle, and its inner diameter is equal to the corresponding height of the 3DN nozzle prefabricated body a truncated circle outer diameter;
  • the outer diameter of the second annular graphite paper stack is equal to the corresponding height truncated inner diameter of the crucible cavity, and the inner diameter is equal to the outer diameter of the graphite support sheet;
  • the third annular graphite paper stack is used for padding into the flat groove to position the top end of the 3DN nozzle prefabricated body a.
  • each crucible layer is composed of two crucible units, and each crucible unit has a half ring shape, and the two crucible units are connected and fastened by double-headed graphite bolts and nuts, and the layer-to-layer The connection surfaces of the two crucible units are perpendicular to each other.
  • a sinker is provided on the outer wall of each crucible unit, bolt holes are provided on the side walls of the sinker at the ends of the outer walls of the two crucible units in each crucible layer, and double-ended graphite bolts pass through the two bolts at the same time. hole, and fasten its two ends respectively by two said nuts.
  • the inner side of the graphite support sheet is inserted into the graphite column, and is supported by a graphite pin radially inserted into the graphite column at its lower part.
  • the difference between the inner diameter of the truncated circle at each height of the crucible and the outer diameter of the truncated circle at the corresponding height of the 3DN nozzle preform a is 50-100 mm;
  • the graphite ring wall is composed of three parts, and each part is one-third of the ring, which form a complete ring after being combined.
  • the height difference between the graphite ring wall and the 2D part b is 5-10mm;
  • the inner diameter of the graphite ring plate is 1 to 3 mm smaller than the outer diameter of the small end of the 3DN nozzle prefabricated body a;
  • the ratio of the diameter of the graphite column to the inner diameter of the small end a of the 3DN nozzle preform is 1:2-5;
  • the material density of the cross plate is 1.9-2.0g/cm 3 ;
  • the wall thickness of the graphite inner support is 8-15 mm, and the outer diameter is 50-100 mm smaller than the inner diameter of the truncated circle of the corresponding height of the 3DN nozzle prefabricated body a.
  • the present invention also provides a method for fused siliconizing the inside and outside of 2D and 3DN ceramic matrix composite components, based on the above-mentioned 2D and 3DN ceramic matrix composite component internal and external powder fused siliconizing tooling, which is special in that it includes the following step:
  • the 2D part b and the 3DN nozzle preform a in the 2D and 3DN ceramic matrix composite components are processed by chemical vapor deposition process, both of which have a density of 1.5-1.6g/cm 3 ;
  • 2D part b and 3DN nozzle prefabricated body a are processed and assembled online to form 2D, 3DN ceramic matrix composite component prefabricated body;
  • the inner diameter of the second annular graphite paper stack is equal to the outer diameter of the graphite support, and the outer diameter is equal to the corresponding height of the 3DN nozzle prefabricated body a truncated circle inner diameter;
  • the furnace is turned on to open the crucible layer from top to bottom, and all graphite paper stacks and residual materials after the reaction are cleaned up to obtain siliconized 2D and 3DN ceramic matrix composite components.
  • step 3) is specifically:
  • step B) the particle size of the silicon powder and silicon carbide powder before mixing is greater than 800 mesh, and the purity is 99.9%;
  • step 2.7 the SiC sand filled into the 3DN nozzle prefabricated body a is 5-10mm lower than the lower edge of the 3DN nozzle prefabricated body a;
  • step 2.8 the mixed powder filled into the 3DN nozzle preform a is 5-10mm higher than the upper edge of the 2D part b.
  • the 2D, 3DN ceramic matrix composite material assembly internal and external powder fusion siliconizing tooling and method provided by the present invention rely on production tasks, adopt 2D parts b pre-tooling protection, internal and external powder filling and other technical methods, and cooperate with special tooling Realize the RMI process of large-size circular cross-section ceramic matrix composite components near net size (that is, the size is almost unchanged before and after treatment), which reduces the difficulty of subsequent processing and assembly, reduces production costs, and shortens the production cycle.
  • the 2D, 3DN ceramic matrix composite component internal and external powder fusion siliconizing tooling and method provided by the present invention physically isolate the 2D parts from the high-temperature melt by designing the graphite protection tooling for the bottom 2D parts, and the components cannot be infiltrated.
  • the high-temperature infiltrated 2D parts are protected, which improves the flexibility of component structure design and process feasibility.
  • the 2D, 3DN ceramic matrix composite material component internal and external powder fusion siliconizing tooling and method provided by the present invention through the graphite inner support installed on the graphite column in the middle, ensure the thickness of the internal modified parts embedded in the powder, and improve the The uniformity of densification is improved, and the use of the graphite inner support reduces the amount of internal buried powder and the gravity effect brought by it, and improves the ability to control the deformation of the component during the high-temperature modification process, and utilizes the embedded graphite in the graphite inner support.
  • Silicon carbide sand which improves the temperature uniformity inside the crucible
  • the 2D and 3DN ceramic matrix composite material assembly internal and external powder fusion siliconizing tooling and method provided by the present invention control the deformation of the large end roundness of the 3DN nozzle prefabricated body a by designing the composite material deformation control tooling, reducing the The risk of deformation of composite components during high temperature modification is eliminated.
  • Fig. 1 is the structural representation of 2D, 3DN ceramic matrix composite material components to be processed in the present invention
  • Fig. 2 is a structural schematic diagram of placing 2D and 3DN ceramic matrix composite components inside and outside the 2D and 3DN ceramic matrix composite components of the present invention
  • Fig. 3 is a schematic diagram of the structure of the 2D and 3DN ceramic matrix composite components inside and outside the embedded powder fusion siliconizing tooling of the present invention
  • Fig. 4 is a structural schematic diagram 2 of the 2D and 3DN ceramic matrix composite components inside and outside of the present invention.
  • Fig. 5 is a schematic diagram of the structure of the 2D and 3DN ceramic matrix composite components inside and outside the powder-embedded fusion siliconizing tooling III.
  • the composite material deformation control tooling and graphite column are not shown in the figure;
  • Fig. 6 is a schematic diagram 4 of the structure of the 2D and 3DN ceramic matrix composite components inside and outside the powder-embedded fusion siliconizing tooling of the present invention, and the composite material deformation control tooling, graphite column and graphite inner support are not shown in the figure;
  • Fig. 7 is a schematic diagram of the structure of the 2D and 3DN ceramic matrix composite components inside and outside the embedded powder fusion siliconizing tooling five, in which one of the crucible unit of the first crucible layer and the three components of the graphite ring wall are not shown in the figure one;
  • Fig. 8 is a schematic diagram of the structure of the 2D and 3DN ceramic matrix composite components inside and outside the powder-embedded fused siliconizing tooling VI of the present invention. The figure does not show one of the crucible units of each crucible layer and one of the three components of the graphite ring wall. one;
  • Fig. 9 is a structural schematic diagram VII of the 2D, 3DN ceramic matrix composite material assembly inside and outside the embedded powder melting siliconizing tooling, the crucible part in the figure only shows one of the crucible units of the first crucible layer;
  • Fig. 10 is a schematic structural view of the 2D component graphite protection tooling in the 2D and 3DN ceramic matrix composite material components of the present invention, which are buried inside and outside the powder fusion siliconizing tooling;
  • Fig. 11 is the temperature curve diagram of the preparation process in the embodiment of the present invention.
  • Fig. 12 is an X-ray non-destructive detection diagram of a product obtained by a fusion siliconizing reaction in an embodiment of the present invention.
  • Fig. 13 is a CT non-destructive testing diagram of a truncated circle of a product obtained by a fusion siliconizing reaction in an embodiment of the present invention, and c and d represent CT nondestructive testing diagrams of a truncated circle at different heights;
  • a-3DN nozzle prefabricated body b-2D parts, b 1 - corner box, b 2 - end flange;
  • a 2D, 3DN ceramic matrix composite material component internal and external powder-embedded fusion silicon infiltration tooling including crucible, 2D parts graphite protection tooling 13, graphite column 14, graphite support sheet 15, graphite inner support 12 and composite material deformation control tooling 5, and The second annular graphite paper stack, the third annular graphite paper stack and 3 first annular graphite paper stacks.
  • the crucible adopts a combined graphite crucible (conventional mechanical processing method), which is composed of 4 graphite crucible layers. , 4 crucible layers, the shape of the crucible cavity matches the shape of the 2D and 3DN ceramic matrix composite components, and the inner diameter of the cut circle at each height of the crucible cavity is greater than the corresponding height of the 2D and 3DN ceramic matrix composite components. ; Of course, the number of layers of the crucible and the shape of the inner cavity of the crucible can be changed according to the shape of the component to be processed.
  • each crucible layer is composed of 2 crucible units, and each crucible unit has a half ring shape (that is, a circular ring), and the two crucible units are connected and fastened by double-headed graphite bolts and nuts , the connection surfaces of the two crucible units between the layers are orthogonal to each other.
  • connection and fastening method of double-headed graphite bolts and nuts is as follows: a sinker is provided on the outer wall of each crucible unit, and bolt through holes are provided on the side walls of the sinker at the ends of the outer walls of the two crucible units in each crucible layer.
  • the head graphite bolt passes through the two bolt holes at the same time, and the two ends of the bolt are respectively fastened by the two nuts.
  • the difference between the inner diameter of the truncated circle at each height of the crucible and the outer diameter of the truncated circle at the corresponding height of the 3DN part a is generally selected in the range of 50-100 mm.
  • the graphite protective tooling 13 of the 2D parts is arranged at the bottom of the crucible cavity, including the graphite ring wall, the graphite ring plate arranged at the inner bottom of the graphite ring wall, and the graphite ring wall and the bottom of the graphite ring plate are correspondingly arranged and evenly distributed along the circumference 9 outrigger groups;
  • the inner diameter of the graphite ring plate is greater than the outer diameter of the graphite column 14 and less than the outer diameter of the 2D part b in the 2D and 3DN ceramic matrix composite assembly;
  • the height of the graphite ring wall is higher than that of the 2D part b height; the area between adjacent leg groups is used as a slurry via hole;
  • the 2D part b includes a corner box b 1 for reinforcement and an end flange b 2 ; in order to prevent the 2D part b from being corroded by silicon melt, the
  • the graphite ring wall is composed of three parts, each
  • the height difference between the graphite ring wall and the 2D part b is 5-10 mm; the inner diameter of the graphite ring plate is 1-3 mm smaller than the outer diameter of the small end of the 3DN nozzle prefabricated body a; there are 9 outrigger groups in total. 9 slurry via holes are formed at the bottom of the graphite protective tooling of 2D parts to reduce the accumulation of liquid silicon and solve the problem of bonding.
  • the circumferential distance between adjacent leg groups is 80-120mm.
  • the graphite column 14 is arranged in the cavity of the crucible, which is coaxial with the crucible, and its bottom end is in contact with the inner bottom surface of the crucible through the graphite ring plate, and its diameter is smaller than that of the 3DN nozzle preform a in the 2D and 3DN ceramic matrix composite components.
  • the inner diameter of the small end is provided with a cross groove at the top; the ratio of the diameter of the graphite column 14 to the inner diameter of the small end of the 3DN nozzle prefabricated body a is 1:2 ⁇ 5, and the diameter of the graphite column 14 here is 180mm.
  • the graphite inner support 12 is a variable-diameter ring with a bottom hole.
  • its outer diameter is smaller than the inner diameter of the 3DN nozzle prefabricated body a. The difference is 50-100 mm.
  • the graphite inner support 12 is sleeved on the graphite column 14 through the bottom circular hole. The diameter of the bottom circular hole is equal to the outer diameter of the graphite column 14, and its wall thickness is 8-15 mm.
  • the graphite inner support 12 is supported by the graphite support sheet 15; the diameter of the small end of the graphite inner support 12 is 290mm, the diameter of the large end is 400mm, the height is 150mm, the diameter of the bottom circular hole is 188mm, and the wall thickness is 8mm.
  • the composite material deformation control tooling 5 is a cross plate.
  • the material The material is the same as that of 2D and 3DN ceramic matrix composite components, that is, continuous fiber reinforced silicon carbide ceramic matrix composite material.
  • its density needs to be greater than that of 2D and 3DN ceramic matrix composite material components.
  • the material density is 1.9-2.0g/cm 3 , the middle part of the cross plate is embedded in the cross groove, and the lower surface of each end is provided with a flat groove 16;
  • the first annular graphite paper lamination is a multilayer (such as 3 to 5 layers) graphite paper stack, and an annular graphite paper lamination bonded as one by scotch tape (one side of each single-layer graphite paper is pasted with an industrial adhesive tape to increase Strength); 3 first annular graphite paper laminates are respectively laid between the inner cavity of the crucible and the outer wall of the 3DN nozzle prefabricated body a, and are used as layered baffles for the filler; the outer surface of each first annular graphite paper laminate The diameter is equal to the corresponding height truncated inner diameter of the crucible cavity, and its inner diameter is equal to the corresponding height truncated outer diameter of the 3DN nozzle preform a; the outer diameter of the second annular graphite paper stack is equal to the corresponding height truncated inner diameter of the crucible cavity, and the inner diameter is equal to The outer diameter of the graphite support sheet; the third annular graphite paper stack is used for
  • the present invention also provides a 2D, 3DN ceramic matrix composite component internal and external powder fusion siliconization method, based on the above-mentioned 2D, 3DN ceramic matrix composite component internal and external powder fusion siliconization tooling, including the following steps:
  • A1 Use chemical vapor deposition process to process 2D part b and 3DN nozzle preform a (machined into semi-finished product) in 2D and 3DN ceramic matrix composite components, both of which have a density of 1.5-1.6g/cm 3 ;
  • boron nitride and absolute ethanol evenly at a mass ratio of 2 to 4:1, evaporate part of the absolute ethanol at 45 to 78°C until the mixture becomes a paste, and obtain boron nitride slurry as an anti-sticking material; preferably The ratio of boron nitride to absolute ethanol is 2:1;
  • the mixed powder Mix the silicon powder and silicon carbide powder evenly according to the mass ratio of 1:1 ⁇ 1.5 to obtain the mixed powder; in order to make the penetration uniform, the particle size of the silicon powder and silicon carbide powder before mixing is greater than 800 mesh, and the purity is 99.9 %; the sieve fineness of the mixed powder should still be greater than 800 mesh;
  • the modified density of the 3DN nozzle part (3DN part a) in the assembly in this example is 2.20g/cm 3 , and it can be seen from Figures 12 and 13 that the density of the modified 2D and 3DN ceramic matrix composite components is uniform .

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Abstract

La présente invention concerne un outil et un procédé pour l'incorporation interne et externe de poudre et l'infiltration de silicium fondu d'un composant composite 2D, 3DN à matrice céramique et vise à résoudre les problèmes techniques selon lesquels, lors de la préparation, au moyen d'un procédé RMI, d'une préforme de buse 3DN de grande dimension, présentant une section transversale circulaire dans le composant composite 2D, 3DN à matrice céramique, une partie 2D est facilement érodée par une masse fondue de silicium pour provoquer une dégradation des performances, la modification à haute température de la préforme de buse 3DN au niveau de la position de surface de contact entre la partie 2D et la préforme de buse 3DN est difficile, le procédé de densification globale du composant est difficile et la préforme de buse 3DN est facilement déformée pendant un processus de modification. L'outil comprend un creuset, un outil de protection en graphite de partie 2D, une colonne de graphite, une pièce support en graphite, un support interne en graphite, un outil de régulation de déformation composite et (N-1) premières couches annulaires d'empilement de papier en graphite, N étant supérieur ou égal à 3. Le procédé est mis en oeuvre à l'aide de l'outil; des procédés de traitement, tels qu'une protection de préoutil de la partie 2D b et l'incorporation et le remplissage interne et externe de poudre, sont utilisés en combinaison avec un outil spécifique, de telle sorte que le processus RMI de dimension presque nette d'un composant composite à matrice céramique de grande dimension présentant une section transversale circulaire est mis en oeuvre, ce qui permet de réduire la difficulté de traitement et d'assemblage ultérieurs.
PCT/CN2022/096447 2021-11-05 2022-05-31 Outil et procédé pour l'incorporation interne et externe de poudre et l'infiltration de silicium fondu d'un composant composite 2d, 3dn à matrice céramique WO2023077790A1 (fr)

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CN115339000B (zh) * 2022-07-25 2025-01-07 西安鑫垚陶瓷复合材料股份有限公司 一种陶瓷基复合材料喷管构件高温改性后校型工装及方法

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